吸电子基团对席夫碱及其钯配合在抑菌及催化活性方面的影响

报道了2, 6-二异丙基苯胺缩苯甲醛或2, 4-二氯苯甲醛席夫碱(L1和L2)及其钯配合物(1和2)的合成, 并通过元素分析、红外光谱、X-射线单晶衍射等方法对席夫碱配体及配合物进行了表征。通过与已报道的席夫碱L1及其钯配合物1结构相比较, 发现引入吸电子取代基合成的一个新的席夫碱及其钯配合(L2和2)对抑菌及催化活性有较大影响。抑菌活性试验表明, 配体及配合物均具有良好的抑菌活性, 配合物相对于配体具有更好的抑菌效果, 配体苯环上的吸电子取代基能有效提高抑菌活性。研究了两组配合物(1和2)对溴代苯和丙烯酸Heck交叉偶联生成苯丙烯酸的催化性能, 考察了不同反应因素(缚酸剂种类、反应温度及溶剂)对该反应的影响, 确定了反应的最佳条件;催化实验结果显示吸电子基团的引入增加了钯配合物的空间位阻效应进而降低其催化活性。     

PMBP缩磺胺席夫碱及其铜配合物的合成与抑菌活性

4-酰基吡唑啉酮类化合物是一类重要的有机配体.其所具有的酮式和烯醇式异构体并存且含有多个配位原子的特性使得该类化合物在与金属离子配位时存在多种配位方式,从而形成单核、同双核、异双核和多核等金属配合物[1-5].     

开链冠醚席夫碱-稀土配合物的合成、表征及抑菌活性研究

合成了三个新型开链冠醚席夫碱-稀土离子三元配合物RE(H2L)(Mq)(NO3)3,其中RE=Nd3 、Er3 、Yb3 ,配体H2L=N,N′-双(邻羟苯亚甲基)-3,6-二氧杂-1,8-二氨基辛烷,Mq为8-羟基喹哪啶。采用元素分析、IR、UV-Vis、热重-差热分析(TG-DTG)等手段对配合物的组成结构进行了表征。抑菌活性实验表明,三种配合物对大肠杆菌有很好的抑菌效果,对金黄色葡萄球菌的抑菌效果较弱。     

对-氨基二甲基苯胺缩PMBP席夫碱及其配合物的合成、表征和抑菌活性

对-氨基二甲基苯胺缩PMBP席夫碱及其配合物的合成、表征和抑菌活性     

水杨醛缩对氨基水杨酸席夫碱及稀土配合物的合成、表征与抑菌活性

以水杨醛和对氨基水杨酸反应制得水杨醛缩对氨基水杨酸席夫碱,并以此席夫碱为配体与水合醋酸稀土盐反应,合成了新的稀土配合物.通过元素分析、摩尔电导、IR、1H-NMR等测试技术对其结构进行了表征:配体与稀土离子按照2∶1进行配位,中心金属离子的配位数为6,组成为[C_(28)H_(20)N_2O_8RE]·2H_2O,其中RE=(La,Ce,Pr,Gd,Dy,Er).抑菌实验初步表明,合成的席夫碱及其配合物对实验选用的细菌有不同程度的抑制活性,而且稀土配合物的抑菌活性更突出.     

聚席夫碱钯（Ⅱ）配合物对芳香族硝基化合物加氢反应的催化性能

以交联聚席夫碱钯的配合物作为催化剂，对芳香族硝基化合物催化加氢性能进行了研究。该催化剂在常温、常压下可使硝基苯１００％催化氢化为苯胺。对某些芳香族硝基化合物转化为相应胺的产率也可达９０％以上。此催化剂性能稳定，重复使用８０次仍具有一定催化活性。     

氨基酸席夫碱镍、钴配合物的合成、晶体结构与抑菌活性

合成了1-苯基-3-甲基-4-对氯苯甲酰基-5-吡唑啉酮缩L-苯丙氨酸甲酯Schiff碱Ni(Ⅱ)、Co(Ⅱ)配合物[NiL_2](CH_3OH)(1)和[CoL_2](CH_3OH)(2)。用元素分析、红外光谱和X-射线单晶结构进行了表征,配合物1和2的晶体结构都同时含有两个独立子单元及一个游离的甲醇分子,各子单元都形成六配位的八面体结构。采用琼脂扩散法测定了配体和配合物对大肠杆菌、金黄色葡萄球菌抗菌活性,结果表明配合物2对大肠杆菌的抑制作用最强。     

乙二胺-2-吡啶甲醛席夫碱钯配合物的制备、表征及其催化性能研究

利用2-吡啶甲醛和乙二胺制得乙二胺-2-吡啶甲醛席夫碱配体,再与钯盐作用制得乙二胺-2-吡啶甲醛席夫碱钯配合物.运用红外光谱、核磁共振、质谱、元素分析、ICP等分析手段对乙二胺-2-吡啶甲醛席夫碱配体及其钯配合物进行了表征,提出了乙二胺-2-吡啶甲醛席夫碱钯配合物的结构,并对其在Heck反应中的催化性能进行了研究.     

乙二胺-2-吡啶甲醛席夫碱钯配合物的制备、表征及其催化性能研究

摘要：本文利用2-吡啶甲醛和乙二胺制得乙二胺-2-吡啶甲醛席夫碱配体,再与钯盐作用制得乙二胺-2-吡啶甲醛席夫碱钯配合物。运用红外光谱、核磁共振、质谱、元素分析、ICP等分析手段对乙二胺-2-吡啶甲醛席夫碱配体及其钯配合物进行了表征,提出了乙二胺-2-吡啶甲醛席夫碱钯配合物的结构,并对其在Heck反应中的催化性能进行了研究。     

PMBP缩2-萘胺席夫碱及其铜(Ⅱ)配合物的合成与抑菌活性

合成了1-苯基-3-甲基-4-苯甲酰基-吡唑啉酮-5(PMBP)缩2-萘胺席夫碱(HL)及其铜(Ⅱ)配合物,由元素分析、络合滴定法、质谱和摩尔电导值确定配合物的组成为[CuL2],通过核磁共振氢谱、红外光谱、热重谱和液相色谱-质谱联用技术对配体和配合物的结构进行了表征,同时还对目标化合物的抑菌活性进行了初步考察。结果表明:配体和配合物对受试的4个菌种均有不同程度的抑菌活性,抑菌能力配合物强于配体,呈现浓度效应,在浓度为3.0 mg.mL-1时最大直径可达14.9 mm。     

新型水杨醛衍生物基Schiff碱的合成及其抑菌活性

以(取代)水杨醛、间(对)羧基苯胺和氨基甲酰肼为原料,分别采用冰浴法合成了4-(二乙基氨基)水杨醛-3-羧基苯胺(3a),4-(二乙基氨基)水杨醛-4-羧基苯胺(3b)和水杨醛-3-羧基苯胺(3c);采用固相法合成了4-(二乙基氨基)水杨醛-氨基甲酰肼(3d);采用水浴回流法合成了3,5-二溴水杨醛-4-羧基苯胺(3e)和2-羟基-1-萘甲醛-4-羧基苯胺(3f),3a~3f均为新化合物,其结构经1H NMR,IR,ESI-MS和元素分析表征。研究了3a~3f对大肠杆菌、金黄色葡萄球菌及欧文氏草生杆菌的抑菌活性。结果表明:3a~3f对受试菌种均有一定的抑菌活性,其中3e的抑菌活性最好。     

(聚酰胺-胺)-水杨醛席夫碱树枝状大分子钯配合物的合成、表征及催化性能

首先通过发散法合成出1.0G～5.0G聚酰胺-胺树枝状大分子PAMAM;然后利用氨基与醛的脱水缩合反应,用水杨醛对大分子进行修饰合成出(聚酰胺-胺)-水杨醛席夫碱树枝状大分子配体PAMAMSA;再通过PAMAMSA与氯钯酸锂在甲醇中反应制得一系列钯配合物PAMAMSA-Pd.用红外光谱、核磁共振谱、热重-差热法对所合成的材料结构组成进行了表征与确证.研究了在纯水介质中PAMAMSA-Pd作为催化剂前躯体对碘代苯及其衍生物与丙烯酸Heck交叉偶联反应的催化性能,并比较了钯配合物和PdCl2的催化活性,结果表明树枝状大分子催化剂显示出良好的催化活性,其中1.0G PAMAMSA-Pd和5.0G PAMAMSA-Pd的活性较高.     

Syntheses,Crystal Structures,and Antibacterial Activities of Four Schiff Base Complexes of Copper and Zinc

Four Schiff base complexes, [Cu₂(L1)₂(μ‐NCS)₂] ( 1 ), [Cu₂(L2)₂(μ‐N₃)₂] ( 2 ), Cu[Cu(CH₃COO)(L3)]₂ ( 3 ), and [Zn{Zn(C₃H₄N₂)(L3)}₂(NO₃)](NO₃) ( 4 ) (where L1 = 2‐[(pyridin‐2‐ylmethylimino)methyl]phenol, L2 = 1‐[(pyridin‐2‐ylmethylimino)methyl]naphthalen‐2‐ol, and L3 = bis(salicylidene)‐1, 3‐propanediamine), were synthesized and characterized by elemental analyses, infrared spectroscopy, and single crystal X‐ray determinations. Both 1 and 2 are structurally similar di‐nuclear complexes, which are located at crystallographic inversion centers (with the center of the central Cu₂N₂ ring). In 1 , each copper atom has a slightly distorted square pyramidal configuration, coordinated by two nitrogen atoms and one oxygen atom from L1 and another two terminal nitrogen atoms from two bridging thiocyanate anions. The Cu···Cu separation is 3.466(3) Å. The structure of 2 is similar to that of 1 , with Cu···Cu separation of 3.368(2) Å. Both 3 and 4 are linear tri‐nuclear complexes. In 3 , the central Cu²⁺ ion is located on an inversion centre and has a distorted octahedral coordination involving four bridging O atoms from two Schiff base ligands (L3) in the equatorial plane and one O atom from each bridging acetate group in the axial positions. The coordination around the terminal Cu²⁺ ions is irregular‐square pyramidal, with two O and two N atoms of L3 in the basal plane and one O atom from an acetate group in the apical position. The acetate bridges linking the central and terminal Cu²⁺ ions are mutually trans. The Cu···Cu separation is 3.009(3) Å. In 4 , the coordination configuration of the central and the terminal zinc atoms are similar to that of the 3 , with Zn···Zn separation of 3.153(4) Å. The three Schiff bases and the corresponding three copper complexes exhibit good antibacterial properties, while the zinc complex 4 has nearly no.     

Syntheses,Crystal Structures and Antibacterial Activities of Two Heterocyclic Schiff Base Compounds

Two heterocyclic Schiff bases were synthesized via the condensation reactions of primary amines with carbonyl compounds. 2-[(4-pyridylmethylene)-amino] phenol(compound 1) was synthesized by the interaction of 4-pyridinecarboxaldehyde with o-aminophenol in ethanol solvent; N,N‘-bis(3-(furan-2-yl)allylidene)benzene-1,4-diamin(compound 2) was synthesized by the interaction of 3-(2-furyl)acrolein with p-phenylenediamine in ethanol medium. The compounds were characterized by elemental analysis, IR, MS and single-crystal X-ray diffraction. Compound 1(C12H10N2O) crystallizes in the monoclinic system, space group P21/c with a = 7.0771(7), b = 7.2820(7), c = 19.849(2),β= 96.3390(10)°, V = 1016.66(17) ?3, Z = 4, Mr = 198.22, Dc = 1.295 g/cm3, F(000) = 416, GOOF = 1.060, μ= 0.085 mm-1, the final R = 0.0371 and wR = 0.0929 for 1497 observed reflections with I 2σ(I). Compound 2(C20H16N2O2) crystallizes in the orthorhombic system, space group Fdd2 with a = 26.344(15), b = 48.50(3), c = 5.293(3), V = 6764(7) ?3, Z = 16, Mr = 316.35, Dc = 1.243 g/cm3, F(000) = 2656, GOOF = 1.043, = 0.081 mm-1, the final R = 0.0526 and wR = 0.1267 for 2059 observed reflections with I 2σ(I). 1 and 2 molecules are connected through hydrogen bonds to generate a 2D network and a 1D chain structure, respectively. The preliminary antibacterial activity results showed that the title compounds display excellent antibacterial activities to Escherichia coli, Staphylococcus aureus and Bacillus subtilis.     

Synthesis and Biological Activities of Alkyl Substituted Triazolethione Schiff Base

Eight Schiff bases have been synthesized using 3‐alkyl‐4‐amino‐1,2,4‐triazole‐5‐thione and substituted benzaldehyde as starting materials. The structures of the compounds have been confirmed by ¹H NMR, IR and elemental analysis and their biological activities to five vegetable pathogens have been tested. The results showed that they exhibited good fungicidal activities.     

1-甲基-2-咪唑醛缩甘氨酸Schiff碱配合物的合成与抑菌活性

以1-甲基-2-咪唑醛和甘氨酸缩合的Schiff碱为配体,合成了4种新的过渡金属配合物[M(C7N3H8O2)(H2O)n]Cl O4(M=Co,Ni,Cu,Zn).经元素分析、摩尔电导率测定、红外光谱、电子光谱和热重分析确证配合物的组成和结构.初步抑菌活性实验表明,合成的配合物对多种菌株有明显的抑菌活性.     

Synthesis,Characterization, and Antimicrobial Activity oF The Ligand 3-Methylpyrazole- 4-Carboxaldehyde Thiosemicarbazone and Its Pd(II) Complex

Abstract

The synthesis and characterization of a new palladium(II) complex [Pd(MePhPzTSC)₂] and its corresponding ligand 3-methylpyrazole-4-carboxaldehyde thiosemicarbazone (MePhPzTSC) are described. The bidentate ligand is coordinated to Pd(II) through the azomethine nitrogen atoms and sulfur in the form of thiol by deprotonation of the NH-C = S. The antimicrobial activity of these new compounds was evaluated against gram-negative (Escherichia coli, Klebsiella pneumoniae, and Pseudomonas aeruginosa) and gram-positive (Staphylococcus aureus and Bacillus thuringiensis) bacteria and two yeast strains (Candida albicans and Saccharomyces cerevisiae). Coordination of the ligand to the metallic ion showed improved antimicrobial activity compared to the free ligand. For the gram-positive bacteria the antimicrobial activity of the complex was higher than that of the positive control used.

[Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the following free supplemental files: Additional figures and tables]     

嫁接型席夫碱配合物的制备及其催化性能

应用超声波技术在温和条件下以氯丙基三甲氧基硅烷为偶联剂, 制得了嫁接过渡金属Zn, Cu, Fe和Co的N,N-双水杨醛缩二乙烯三胺席夫碱配合物[SiO₂-M(NNOO)], 并与传统加热搅拌法制得的样品的物性和催化性能做了比较. 应用IR和UV-Vis谱学技术对其进行了初步表征, 结果表明, 两种方法制得的嫁接型配合物的红外光谱均呈现出胺基和席夫碱相应基团的特征吸收, 配体和配合物红外和紫外光谱之间的差别表明配合物结构的存在. 将所制得的样品在苯乙烯选择氧化制苯甲醛反应中进行了催化性能的测试, 考察了反应时间和催化剂对苯乙烯转化率和选择性的影响, 结果表明苯乙烯转化率均在90%以上, 苯甲醛选择性最高可达93.5%, 产物选择性与反应时间和催化剂中过渡金属的类型均有关系.